CN112175652A - Emulsion bed enhanced reaction system and method for direct coal liquefaction - Google Patents
Emulsion bed enhanced reaction system and method for direct coal liquefaction Download PDFInfo
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/06—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal by destructive hydrogenation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/20—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
- B01J8/22—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G1/00—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal
- C10G1/08—Production of liquid hydrocarbon mixtures from oil-shale, oil-sand, or non-melting solid carbonaceous or similar materials, e.g. wood, coal with moving catalysts
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G7/00—Distillation of hydrocarbon oils
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4006—Temperature
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/40—Characteristics of the process deviating from typical ways of processing
- C10G2300/4012—Pressure
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/70—Catalyst aspects
Abstract
The invention provides a system and a method for an emulsion bed enhanced reaction for direct coal liquefaction, which comprises the following steps: the feeding unit is used for preparing coal slurry and conveying the coal slurry and hydrogen; the emulsion bed liquefaction unit is connected with the feeding unit and is used as a place for carrying out liquefaction reaction on the coal slurry and hydrogen, and the liquefaction reaction product is separated and rectified to obtain light fraction and distillate oil; the emulsified bed hydrogenation unit is connected with the emulsified bed liquefaction unit and is used for carrying out catalytic hydrogenation reaction on the light fraction and the distillate oil to obtain a hydrogen-donating solvent and product oil; and the micro-interface generator is respectively arranged between the emulsifying bed liquefying unit and between the emulsifying bed hydrogenation unit. The emulsion bed enhanced reaction system and method for direct coal liquefaction provided by the invention solve the problem of low reaction efficiency in the direct coal liquefaction process in the prior art because hydrogen cannot fully react with coal slurry.
Description
Technical Field
The invention relates to the technical field of direct coal liquefaction, in particular to a system and a method for an emulsion bed enhanced reaction for direct coal liquefaction.
Background
The direct coal liquefaction technology has been studied as early as the 19 th century. In 1914, the German chemist Curgis studied the liquefaction of coal under hydrogen pressure, and in the same year, together with Bilviller, patented the test. In 1926, the german law company developed a high-efficiency hydrogenation catalyst, and built a plant for preparing liquid fuel from lignite through high-pressure hydrogenation liquefaction by using the bages method. Before world war II, Germany produces liquid fuel from coal and low-temperature carbonization coal tar, which reaches the annual production level of 1.5Mt in 1938, and the total production capacity reaches 4Mt in the later period of world war II; in 1935 England chemical industry, Bilingham, England, also established a hydrogenation plant for producing liquid fuels from coal and coal tar, 150kt annually. In addition, some laboratories have been built in japan, france, canada, and the united states. After a war, due to the decrease of the price of the petroleum, the coal liquefaction product cannot compete with the natural petroleum economically, and the coal liquefaction product is closed in sequence, even the experimental device stops the test. In the early 60 s, especially in 1973, after the price of petroleum was greatly increased, the direct coal liquefaction work was also regarded and a new series of processes such as solvent refining coal method, exxon hydrogen-donating solvent method, hydrogen coal method, etc. in the united states were developed.
Axens North American Limited had a long history of development and demonstration of direct coal liquefaction technology, originating in the last 60 th century. The development of the direct coal liquefaction technology is based on the industrial hydrogen-oil process and proves that the emulsion bed reactor technology has remarkable universality. These technologies, including hydrogen-oil processes, CTSL (two-stage catalytic liquefaction), and coal/oil hybrid processing, are the leading positions of coal liquefaction technology in the world today.
However, in the conventional reaction process of directly liquefying coal using an emulsion bed reactor, hydrogen gas cannot sufficiently react with coal slurry, and thus reaction efficiency is reduced.
Disclosure of Invention
In view of the above, the invention provides a system and a method for an emulsion bed enhanced reaction for direct coal liquefaction, and aims to solve the problem that the reaction efficiency of coal liquefaction is reduced because hydrogen cannot fully react with coal slurry in the direct coal liquefaction process of the conventional emulsion bed reactor.
In one aspect, the present invention provides an emulsion bed enhanced reaction system for direct coal liquefaction, comprising:
the feeding unit is used for preparing coal slurry and conveying the coal slurry and hydrogen;
the emulsion bed liquefaction unit is connected with the feeding unit and is used as a place for carrying out liquefaction reaction on the coal slurry and hydrogen, and the liquefaction reaction product is separated and rectified to obtain light fraction and distillate oil;
the emulsified bed hydrogenation unit is connected with the emulsified bed liquefaction unit and is used for carrying out catalytic hydrogenation reaction on the light fraction and the distillate oil to obtain a hydrogen-donating solvent and product oil;
and the micro-interface generator is respectively arranged between the emulsion bed liquefaction unit and between the emulsion bed hydrogenation unit and is respectively used for converting the pressure energy of gas and/or the kinetic energy of liquid into bubble surface energy and transmitting the bubble surface energy to hydrogen bubbles before the liquefaction reaction and the catalytic hydrogenation so as to break the hydrogen into micron-sized bubbles with the diameter of micron level, thereby increasing the phase boundary mass transfer area between the hydrogen and the corresponding reactant in the liquefaction reaction and the catalytic hydrogenation processes, simultaneously reducing the thickness of a liquid film, reducing the mass transfer resistance and enhancing the reaction phase boundary mass transfer efficiency and the reaction rate.
Further, in the emulsion bed enhanced reaction system for direct coal liquefaction, the micro-interface generator is selected from one or more of a pneumatic micro-interface generator, a hydraulic micro-interface generator and a gas-liquid linkage micro-interface generator.
Further, in the emulsion bed enhanced reaction system for direct coal liquefaction, the micro-interface generator includes: a first micro-interface generator and a second micro-interface generator; the first micro-interface generator is arranged in the emulsifying bed liquefaction unit, and the second micro-interface generator is arranged between the emulsifying bed liquefaction unit and the emulsifying bed hydrogenation unit.
Furthermore, in the emulsion bed enhanced reaction system for directly liquefying coal, the diameter of the micron-sized bubbles is more than or equal to 1 μm and less than 1 mm.
Further, in the above emulsion bed enhanced reaction system for direct coal liquefaction, the emulsion bed liquefaction unit includes: the inside is provided with first emulsion bed reactor, high temperature separator, low temperature separator, ordinary pressure rectifying column and the rectifying column that reduces pressure of first micro-interface generator.
Further, in the above-mentioned emulsion bed enhanced reaction system for direct coal liquefaction, the hydrogenation unit of the emulsion bed comprises: and the second emulsion bed reactor, the gas-liquid separator and the product fractionating tower are connected with the second micro-interface generator.
Further, in the above emulsion bed enhanced reaction system for direct coal liquefaction, the feed unit includes: a slurry conveying unit for preparing and conveying coal slurry and a gas conveying unit for conveying hydrogen.
Further, in the emulsion bed enhanced reaction system for direct coal liquefaction, the micro-interface generator between the emulsion bed liquefaction unit and the emulsion bed hydrogenation unit is a second micro-interface generator, and the second micro-interface generator is connected with the inlet of the second emulsion bed reactor.
The emulsion bed enhanced reaction system for directly liquefying coal has the beneficial effects that the micro-interface generators are respectively arranged between the emulsion bed liquefying unit and between the emulsion bed hydrogenation unit. The micro-interface generator is used for crushing the hydrogen into micron-sized bubbles with the diameter of more than or equal to 1 mu m and less than 1mm in the micro-interface generator before the liquefaction reaction and the catalytic hydrogenation reaction so as to increase the phase boundary mass transfer area between the hydrogen and the corresponding reactant in the reaction process, reduce the thickness of a liquid film, reduce the mass transfer resistance and improve the mass transfer efficiency between reaction phases, thereby solving the problem of low reaction efficiency in the direct coal liquefaction process due to the fact that the hydrogen cannot fully react with coal slurry in the prior art. Meanwhile, the invention can flexibly adjust the range of the preset operation condition according to different raw material compositions, different product requirements or different catalysts so as to ensure the full and effective reaction, further ensure the reaction rate and achieve the purpose of strengthening the reaction.
Particularly, the emulsion bed liquefaction unit is provided with a high-temperature separation tower, a low-temperature separator, an atmospheric distillation tower and a reduced-pressure distillation tower, and can separate and distill the products of the liquefaction reaction to generate light fraction, distillate oil and hydrogen and simultaneously remove waste and solid residues from the system, so that the reaction efficiency of the system is improved, and the utilization efficiency of resources is increased.
On the other hand, the invention also provides an emulsion bed enhanced reaction method for direct coal liquefaction, which comprises the following steps:
preparing raw material coal into coal slurry, directly feeding the coal slurry into a first emulsion bed reactor, introducing hydrogen into a first micro-interface generator arranged in the first emulsion bed reactor, converting pressure energy of gas and/or kinetic energy of liquid into hydrogen bubble surface energy through the first micro-interface generator, crushing the hydrogen bubbles into micron-sized bubbles with the diameter of micron level, and conveying the micron-sized bubbles into the first emulsion bed reactor to perform liquefaction reaction with the coal slurry;
carrying out gas-liquid separation on a liquefied reaction product in a separator, wherein a liquid phase part forms light fraction and distillate oil through a rectifying tower, the light fraction and distillate oil mixed solution and hydrogen are sent into a second micro-interface generator together, the pressure energy of the gas and/or the kinetic energy of the liquid are converted into the surface energy of hydrogen bubbles through the second micro-interface generator, the hydrogen bubbles are crushed into micron-sized bubbles with the diameter of micron level, the micron-sized bubbles are fused into the mixed solution of the light fraction and the distillate oil to form a gas-liquid emulsification system, and the gas-liquid emulsification system is sent into the second emulsification bed reactor to carry out catalytic hydrogenation reaction;
and separating the catalytic hydrogenation product into product oil and a hydrogen-donating solvent through a fractionating tower.
Further, in the emulsion bed enhanced reaction method for direct coal liquefaction, the diameter of the micron-sized bubbles is not less than 1 μm and less than 1 mm.
Further, in the method for the enhanced reaction of the emulsion bed for the direct coal liquefaction, the reaction temperature of the liquefaction reaction is 400-450 ℃, the pressure is 2-14MPa, the gas-liquid ratio is 100-2000, and the space velocity is 0.7-1.2h-1(ii) a The reaction temperature of the catalytic hydrogenation reaction is 330-380 ℃, the pressure is 5-12MPa, the gas-liquid ratio is 250-700, and the space velocity is 0.5-2h-1。
Compared with the prior art, the emulsion bed enhanced reaction method for direct coal liquefaction has the advantages that hydrogen is crushed into micron-sized bubbles by the first micro-interface generator and the second micro-interface generator, so that the phase boundary mass transfer areas of gas-phase reactants and liquid-phase reactants in an emulsion bed liquefaction unit and an emulsion bed hydrogenation unit in the direct coal liquefaction reaction process are effectively increased, the thickness of a liquid film is reduced, the mass transfer resistance is reduced, the mass transfer efficiency between the gas phase and the liquid phase is enhanced, and the problem of low reaction efficiency in the direct coal liquefaction process due to the fact that hydrogen cannot fully react with coal slurry in the prior art is solved. Meanwhile, the invention can flexibly adjust the range of the preset operation condition according to different raw material compositions, different product requirements or different catalysts so as to ensure the full and effective reaction, further ensure the reaction rate and achieve the purpose of strengthening the reaction.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
fig. 1 is a schematic structural diagram of an emulsion bed enhanced reaction system for direct coal liquefaction according to an embodiment of the present invention.
Detailed Description
Exemplary embodiments of the present invention will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the invention are shown in the drawings, it should be understood that the invention can be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The invention will be described in detail below with reference to the accompanying figure 1 in conjunction with an embodiment.
Referring to fig. 1, an emulsion bed enhanced reaction system for direct coal liquefaction according to an embodiment of the present invention includes: the device comprises a feeding unit 1, an emulsion bed liquefaction unit 3, a micro-interface generator and an emulsion bed hydrogenation unit 4; the feeding unit 1 is used for preparing coal slurry and conveying the coal slurry and hydrogen; the emulsifying bed liquefaction unit 3 is used for carrying out liquefaction reaction on the coal slurry and hydrogen, and separating and rectifying a liquefaction reaction product to obtain distillate oil and light fraction, and the emulsifying bed liquefaction unit 3 is respectively connected with the inlet ends of the feeding unit 1 and the second micro-interface generator 22. The inlet end of the second micro-interface generator 22 is further connected with the feeding unit 1, the outlet end is connected with the emulsion bed hydrogenation unit 4, and the second micro-interface generator is used for receiving the light fraction, the distillate oil, the hydrogen in the liquefied reaction product and the hydrogen conveyed by the feeding unit 1, crushing the hydrogen into micron-sized bubbles with the diameter of more than or equal to 1 μm and less than 1mm, mixing the micron-sized bubbles with the light fraction and the distillate oil to form a gas-liquid emulsion after the crushing is completed, and conveying the gas-liquid emulsion to the emulsion bed hydrogenation unit 4. And the fluidized bed hydrogenation unit 4 is used for carrying out catalytic hydrogenation reaction on the gas-liquid emulsion, and separating and rectifying a product of the gas-liquid emulsion to finally generate a hydrogen-supplying solvent and product oil.
Specifically, the feed unit 1 includes: a hydrogen feeding pipeline 11, a coal pretreatment device 12, a catalyst preparation device 13, a coal slurry preparation device 14 and a coal slurry pump 15. One end of the hydrogen feeding pipeline 11 is externally connected with a hydrogen source, and the other end of the hydrogen feeding pipeline is respectively connected with the emulsifying bed liquefying unit 3, the micro-interface generator and the emulsifying bed hydrogenation unit 4 for hydrogen transportation; the coal pre-processor is connected with the inlet end of the coal slurry preparation device 14 and is used for preparing raw material coal powder; the catalyst preparation device 13 is connected with the inlet end of the coal slurry preparation device 14 and is used for preparing catalyst raw materials into ultrafine-particle catalyst powder; the outlet end of the coal slurry preparation device 14 is connected with the inlet of the coal slurry pump 15 and is used for receiving the raw material coal powder and the catalyst powder, and injecting a hydrogen-supplying solvent into the coal slurry preparation device 14, and mixing the raw material coal powder, the catalyst powder and the hydrogen-supplying solvent to form coal slurry; the outlet end of the coal slurry pump 15 is connected with the emulsifying bed liquefaction unit 3 and is used for conveying the coal slurry prepared by the coal slurry preparation device 14 to the emulsifying bed liquefaction unit 3 for carrying out liquefaction reaction.
When the system is in operation, the liquefied raw coal is dried and pulverized by the coal pretreatment device 12 to produce pulverized coal of a certain particle size. The catalyst raw material is made into the catalyst of ultrafine particles by the catalyst preparation device 13. The coal powder and the catalyst are mixed with a hydrogen-supplying solvent in the coal slurry preparation device 14 to prepare coal slurry, the coal slurry enters the emulsifying bed liquefaction unit 3 after being prepared, and meanwhile, the hydrogen conveying pipeline conveys the hydrogen to the emulsifying bed liquefaction unit 3.
Specifically, the micro-interface generator converts the pressure energy of the gas and/or the kinetic energy of the liquid into the surface energy of the bubbles and transmits the surface energy to the hydrogen bubbles, so that the hydrogen is broken into micron-sized bubbles with the diameter of micron scale. Meanwhile, the micro-interface generator is divided into a pneumatic micro-interface generator, a hydraulic micro-interface generator or a gas-liquid linkage micro-interface generator according to an energy input mode or a gas-liquid ratio; the pneumatic micro-interface generator is driven by gas, and the input gas quantity is far larger than the liquid quantity; the hydraulic micro-interface generator is driven by liquid, and the input air quantity is generally smaller than the liquid quantity; the gas-liquid linkage type micro-interface generator is driven by gas and liquid at the same time, and the input gas amount is close to the liquid amount. In this embodiment, the micro-interface generator includes: a first micro-interface generator 21 and a second micro-interface generator 22; the first micro-interface generator 21 is arranged in the emulsifying bed liquefaction unit 3, the second micro-interface generator 22 is arranged between the emulsifying bed liquefaction unit and the emulsifying bed hydrogenation unit, and the first micro-interface generator 21 and the second micro-interface generator 22 are selected from one or more of a pneumatic micro-interface generator, a hydraulic micro-interface generator and a gas-liquid linkage micro-interface generator.
Specifically, the fluidized-bed liquefaction unit 3 includes: a first emulsion bed reactor 31, a high temperature separator 32, a low temperature separator 33, an atmospheric distillation column 34 and a vacuum distillation column 35; the first micro-interface generator 21 is located inside the first emulsion bed reactor 31, is connected with the hydrogen feeding pipeline 11, and is used for crushing hydrogen into micron-sized bubbles with the diameter of more than or equal to 1 μm and less than 1mm and conveying the micron-sized bubbles into the first emulsion bed reactor 31; the inlet end of the first emulsion bed reactor 31 is respectively connected with the coal slurry pump 15 and the emulsion bed hydrogenation unit 4, and the outlet end of the first emulsion bed reactor 31 is connected with the inlet of the high-temperature separator 32, so as to receive the coal slurry and the hydrogen micron-sized bubbles and serve as a reaction chamber for liquefaction reaction of the coal slurry and the hydrogen micron-sized bubbles; the outlet end of the high-temperature separator 32 is connected with the inlet ends of the low-temperature separator 33 and the normal-pressure rectifying tower 34 respectively, and is used for carrying out gas-liquid separation on the liquefied reaction product to obtain a gas-phase product which enters the low-temperature separator 33 and a liquid-phase product which enters the normal-pressure rectifying tower 34; the outlet end of the low-temperature separation tower is respectively connected with a hydrogen feeding pipeline 11 and an atmospheric distillation tower 34, and is used for receiving the gas-phase product separated from the high-temperature separator 32 and further carrying out gas-liquid separation on the gas-phase product, the generated gas-phase product enters the hydrogen feeding pipeline 11 to be mixed with hydrogen for recycling, part of the waste gas 5 is discharged from the system, and the generated liquid-phase product enters the atmospheric distillation tower; the outlet end of the atmospheric fractionating tower is respectively connected with the second micro-interface separator and the vacuum rectification tower 35, and is used for fractionating the liquid-phase products generated by the high-temperature separator 32 and the low-temperature separator 33 to obtain light fractions which enter the second micro-interface generator 22, and the tower bottom materials enter the vacuum rectification tower 35; the outlet end of the reduced pressure rectifying tower 35 is connected with the inlet end of the second micro-interface generator 22 and is used for removing asphalt and solid from the tower bottom material generated by the atmospheric pressure rectifying tower 34 to obtain distillate oil which enters the second micro-interface generator 22 and the liquefied residue 6 removal system.
Hydrogen enters the first micro-interface generator 21, is crushed into micron-sized bubbles, enters the first emulsion bed reactor 31, and is subjected to a liquefaction reaction with coal slurry entering the first emulsion bed reactor 31, a liquefaction reaction product generated by the first emulsion bed reactor 31 enters the high-temperature separator 32 for gas-liquid separation, a gas-phase product obtained by the separation of the high-temperature separator 32 enters the low-temperature separator 33 for further gas-liquid separation, the gas-phase product obtained by the low-temperature separator 33 is mixed with the hydrogen for recycling, and 5 parts of waste gas are discharged out of the system. Liquid phase products of the high-temperature separator 32 and the low-temperature separator 33 enter the atmospheric distillation tower 34 to separate light fractions, tower bottom materials of the atmospheric distillation tower 34 enter the vacuum distillation tower 35 to remove asphalt and solids, the tower bottom materials of the vacuum distillation tower 35 are liquefaction residues 6, and the liquefaction residues 6 are discharged out of the system. In order to ensure that the residue can be removed smoothly at a certain temperature, the solids content of the residue is generally controlled to 50-55 wt.%. The light fractions and distillate oil generated in the atmospheric distillation tower 34 and the vacuum distillation tower 35 are mixed with hydrogen gas and enter the second micro-interface generator 22.
Specifically, the fluidized-bed hydrogenation unit 4 includes: a second emulsion bed reactor 41, a gas-liquid separator 42 and a product fractionation column 43. Wherein the inlet end of the second emulsion bed reactor 41 is connected with the outlet end of the second micro interface generator 22, and the outlet end thereof is connected with the inlet end of the gas-liquid separator 42, so as to receive the gas-liquid emulsion generated by the second micro interface generator 22 and serve as a catalytic hydrogenation reaction chamber of the gas-liquid emulsion; the outlet end of the gas-liquid separator 42 is respectively connected with the product fractionating tower 43 and the hydrogen feeding pipeline 11, so that the catalytic hydrogenation product is subjected to gas-liquid separation, the obtained gas-phase product and hydrogen are mixed and recycled, the waste part is removed from the system, and the obtained liquid-phase product enters the product fractionating tower 43; the product fractionating tower 43 is further connected to the first emulsion bed reactor 31, and is configured to fractionate the liquid-phase product produced by the gas-liquid separator 42 to obtain the product oil 8 and the circulating solvent 7, and the circulating solvent 7 is circulated to the first emulsion bed reactor 31 to perform the secondary liquefaction reaction.
The second micro-interface generator 22 crushes the hydrogen into micron-sized bubbles and mixes the micron-sized bubbles with the light fraction and the distillate oil to form a gas-liquid emulsion, the gas-liquid emulsion is conveyed to the inside of the second emulsion bed reactor 41, the second emulsion bed reactor 41 is subjected to catalytic hydrogenation for the purpose of improving the hydrogen supply performance of the gas-liquid emulsion, the outlet material of the second emulsion bed reactor 41 enters the gas-liquid separator 42 for gas-liquid separation, the gas-phase product generated by the gas-liquid separator 42 is mixed with the hydrogen for recycling, and 5 parts of the waste gas are discharged out of the system. The liquid phase material produced by the gas-liquid separator 42 enters a product fractionating tower 43, and the product oil 8 and the circulating solvent 7 are fractionated. Wherein the circulating solvent 7 circulates to the first emulsion bed reactor 31 for secondary liquefaction reaction, and the product oil 8 is all gasoline and diesel oil fractions.
In the emulsion bed enhanced reaction system for direct coal liquefaction in this embodiment, the first micro-interface generator 21 is arranged inside the first emulsion bed reactor 31, and the second micro-interface generator 22 is arranged at the inlet end of the second emulsion bed reactor 41, so that hydrogen is broken into micron-sized bubbles with a diameter of micron level in the corresponding micro-interface generator before liquefaction reaction and catalytic hydrogenation reaction, the phase boundary mass transfer area between reactants such as hydrogen and coal slurry in the reaction process is effectively increased, the mass transfer efficiency between reaction phases is improved, and the problem of low reaction efficiency in the direct coal liquefaction process due to insufficient reaction of hydrogen and coal slurry in the prior art is solved.
The following describes the specific method and effect of the system according to the present invention with reference to specific embodiments.
An emulsion bed enhanced reaction method for direct coal liquefaction comprises the following steps:
preparing raw material coal into coal slurry, feeding the coal slurry into a first emulsion bed reactor, and introducing hydrogen into a first micro-interface generator;
the first micro-interface generator is used for crushing the hydrogen into micron-sized bubbles with micron scale, and conveying the micron-sized bubbles into the first emulsion bed reactor to carry out liquefaction reaction with the coal slurry;
carrying out gas-liquid separation on the liquefied reaction product in a separator, wherein a liquid phase part forms a light fraction and a distillate oil through a rectifying tower, and the light fraction and the distillate oil are mixed and then are sent to the interior of the second micro-interface generator together with hydrogen;
the second micro-interface generator is used for crushing the hydrogen into micron-sized bubbles with micron scale, mixing the micron-sized bubbles with the mixture of the light fraction and the distillate oil to form a gas-liquid emulsion, and sending the emulsion to the inside of the second emulsion bed reactor for catalytic hydrogenation reaction;
and separating the catalytic hydrogenation product into product oil and other hydrogen-donating solvents by a fractionating tower.
In the embodiment, the reaction temperature of the liquefaction reaction is 400-450 ℃, the pressure is 2-14MPa, the gas-liquid ratio is 100-2000, and the space velocity is 0.7-1.2h-1。
In the embodiment, the reaction temperature of the catalytic hydrogenation reaction is 330--1。
It can be understood that the range of the preset operation conditions can be flexibly adjusted according to different raw material compositions, different product requirements or different catalysts, so as to ensure the full and effective reaction, further ensure the reaction rate and achieve the purpose of strengthening the reaction. Meanwhile, in the present embodiment, the kind of the catalyst is not particularly limited, and may be one or a combination of several of an iron-based catalyst, a molybdenum-based catalyst, a nickel-based catalyst, a cobalt-based catalyst, and a tungsten-based catalyst, as long as the strengthening reaction can be smoothly performed.
In order to further verify the processing method provided by the invention, the beneficial effects of the invention are further illustrated by combining the examples and the comparative examples.
The following is the liquefaction result of direct liquefaction of an enhanced coal under three different reaction conditions using the preferred embodiment of the present invention.
The first embodiment is as follows:
the reactor temperature: the first emulsion bed reactor is 400 ℃, and the second emulsion bed reactor is 330 ℃.
Reaction pressure: the first emulsion bed reactor is 2MPa, and the second emulsion bed reactor is 5 MPa.
Gas-liquid ratio: a first emulsion bed reactor 100 and a second emulsion bed reactor 250.
Space velocity: the first emulsion bed reactor is used for 0.7h-1Second emulsion bed reactor for 0.5h-1。
Coal slurry concentration: 40/50 (dry coal/solvent, mass ratio).
The addition amount of the catalyst is as follows: liquefaction catalysis aid: 1.0wt% (iron/dry coal).
The addition amount of sulfur: S/Fe =2 (molar ratio).
In this example, the conversion of coal was 82.43%, the oil yield in the product was 52.23%, and the hydrogen consumption was 8.59%.
Example two:
the reactor temperature: the first emulsion bed reactor is 420 ℃, and the second emulsion bed reactor is 350 ℃.
Reaction pressure: the first emulsion bed reactor is 8MPa, and the second emulsion bed reactor is 8 MPa.
Gas-liquid ratio: a first emulsion bed reactor 1000, a second emulsion bed reactor 500.
Space velocity: the first emulsion bed reactor is used for 1.0h-1Second emulsion bed reactor for 1.3h-1。
Coal slurry concentration: 40/50 (dry coal/solvent, mass ratio).
The addition amount of the catalyst is as follows: liquefaction catalysis aid: 1.0wt% (iron/dry coal).
The addition amount of sulfur: S/Fe =2 (molar ratio).
In this example, the conversion of coal was 83.39%, the oil yield in the product was 58.28%, and the hydrogen consumption was 7.10%.
Example three:
the reactor temperature: the temperature of the first emulsion bed reactor is 450 ℃, and the temperature of the second emulsion bed reactor is 380 ℃.
Reaction pressure: the first emulsion bed reactor is 14MPa, and the second emulsion bed reactor is 12 MPa.
Gas-liquid ratio: a first emulsion bed reactor 2000, a second emulsion bed reactor 700.
Space velocity: the first emulsion bed reactor is used for 1.2h-1Second emulsion bed reactor for 2.0h-1。
Coal slurry concentration: 40/50 (dry coal/solvent, mass ratio).
The addition amount of the catalyst is as follows: liquefaction catalysis aid: 1.0wt% (iron/dry coal).
The addition amount of sulfur: S/Fe =2 (molar ratio).
In this example, the conversion of coal was 90.33%, the oil yield in the product was 62.96%, and the hydrogen consumption was 6.76%.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (10)
1. An emulsion bed enhanced reaction system for direct coal liquefaction is characterized by comprising:
the feeding unit is used for preparing coal slurry and conveying the coal slurry and hydrogen;
the emulsion bed liquefaction unit is connected with the feeding unit and is used as a place for carrying out liquefaction reaction on the coal slurry and hydrogen, and the liquefaction reaction product is separated and rectified to obtain light fraction and distillate oil;
the emulsified bed hydrogenation unit is connected with the emulsified bed liquefaction unit and is used for carrying out catalytic hydrogenation reaction on the light fraction and the distillate oil to obtain a hydrogen-donating solvent and product oil;
and the micro-interface generator is respectively arranged between the emulsion bed liquefaction unit and between the emulsion bed hydrogenation unit and is respectively used for converting the pressure energy of gas and/or the kinetic energy of liquid into bubble surface energy and transmitting the bubble surface energy to hydrogen bubbles before the liquefaction reaction and the catalytic hydrogenation so as to break the hydrogen into micron-sized bubbles with the diameter of micron level, so as to increase the phase boundary mass transfer area between the hydrogen and the corresponding reactant in the liquefaction reaction and the catalytic hydrogenation processes, reduce the thickness of a liquid film, reduce the mass transfer resistance and strengthen the reaction phase boundary mass transfer efficiency and the reaction rate.
2. The emulsion bed enhanced reaction system for direct coal liquefaction according to claim 1, wherein the micro-interface generator is selected from one or more of a pneumatic micro-interface generator, a hydraulic micro-interface generator and a gas-liquid linkage micro-interface generator.
3. The emulsion bed enhanced reaction system for direct coal liquefaction according to claim 2, wherein the micro-interface generator comprises: a first micro-interface generator and a second micro-interface generator; the first micro-interface generator is arranged in the emulsifying bed liquefaction unit, and the second micro-interface generator is arranged between the emulsifying bed liquefaction unit and the emulsifying bed hydrogenation unit.
4. The emulsion bed enhanced reaction system for direct coal liquefaction according to claim 1, wherein the diameter of the micro-sized bubbles is 1 μm or more and less than 1 mm.
5. The emulsion bed enhanced reaction system for direct coal liquefaction according to claim 3, wherein the emulsion bed liquefaction unit comprises: the inside is provided with first emulsion bed reactor, high temperature separator, low temperature separator, ordinary pressure rectifying column and the rectifying column that reduces pressure of first micro-interface generator.
6. The emulsion bed enhanced reaction system for direct coal liquefaction according to claim 3, wherein the emulsion bed hydrogenation unit comprises: and the second emulsion bed reactor, the gas-liquid separator and the product fractionating tower are connected with the second micro-interface generator.
7. The emulsion bed enhanced reaction system for direct coal liquefaction according to claim 1, wherein the feed unit comprises: a slurry conveying unit for preparing and conveying coal slurry and a gas conveying unit for conveying hydrogen.
8. The method for the enhanced reaction of the emulsion bed for the direct coal liquefaction is characterized by comprising the following steps of:
preparing raw material coal into coal slurry, directly feeding the coal slurry into a first emulsion bed reactor, introducing hydrogen into a first micro-interface generator arranged in the first emulsion bed reactor, converting pressure energy of gas and/or kinetic energy of liquid into hydrogen bubble surface energy through the first micro-interface generator, crushing the hydrogen bubbles into micron-sized bubbles with the diameter of micron level, and conveying the micron-sized bubbles into the first emulsion bed reactor to perform liquefaction reaction with the coal slurry;
carrying out gas-liquid separation on a liquefied reaction product in a separator, wherein a liquid phase part forms light fraction and distillate oil through a rectifying tower, the light fraction and distillate oil mixed solution and hydrogen are sent into a second micro-interface generator together, the pressure energy of the gas and/or the kinetic energy of the liquid are converted into the surface energy of hydrogen bubbles through the second micro-interface generator, the hydrogen bubbles are crushed into micron-sized bubbles with the diameter of micron level, the micron-sized bubbles are fused into the mixed solution of the light fraction and the distillate oil to form a gas-liquid emulsification system, and the gas-liquid emulsification system is sent into the second emulsification bed reactor to carry out catalytic hydrogenation reaction;
and separating the catalytic hydrogenation product into product oil and a hydrogen-donating solvent through a fractionating tower.
9. The emulsion bed enhanced reaction method for direct coal liquefaction according to claim 7, wherein the diameter of the micro-sized bubbles is 1 μm or more and less than 1 mm.
10. The method as claimed in claim 7, wherein the liquefaction reaction has a temperature of 400-450 ℃, a pressure of 2-14MPa, a gas-liquid ratio of 100-2000, and a space velocity of 0.7-1.2h-1(ii) a The reaction temperature of the catalytic hydrogenation reaction is 330-380 ℃, the pressure is 5-12MPa, the gas-liquid ratio is 250-700, and the space velocity is 0.5-2.0h-1。
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| CN1587351A (en) * | 2004-07-30 | 2005-03-02 | 神华集团有限责任公司 | Method for directly liquefying coal |
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